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Nanofiber Webs from Electrospinning
Timothy H. Grafe, Kristine M. Graham
1. CHARACTERISTICS OF SMALL FIBERS IN AIR FILTRATION THEORY
Small fibers in the submicron range, in comparison with larger ones, are well known to provide better filter efficiency at the same pressure drop in the interception and inertial impaction regimes. W.C. Hinds shows such effect by assuming non-slip flow at fiber surface . While smaller fiber size leads to higher pressure drop, interception and inertial impaction efficiencies will increase faster, more than compensating for the pressure drop increase. Thus, in the particle size of interest, i.e., from submicron and up, better filter efficiency can be achieved at the same pressure drop, or conversely, the same filter efficiency at lower pressure drop can be achieved with smaller fiber sizes. For nanometer-scale fibers, a second factor has to be taken into account: the effect of slip flow at the fiber surface . Filtration theory generally relies on an assumption of continuous flow around the fiber, with a no-slip condition at the fiber surface. The theory starts to become less valid when the scale of the fiber becomes small enough that the molecular movements of the air molecules are significant in relation to the size of the fibers and the flow field. Using a slipflow model at the fiber surface can extend the useful range of continuous flow theory. The Knudsen number is used to describe the importance of the molecular movements of air molecules at the fiber surface to the overall flow field. The Knudsen number can be written as
Donaldson Company Inc. Minneapolis, MN, USA
Elecotrospun nanofibers, with fiber diameters of 0.25 microns have been used in industrial, consumer and defense filtration applications for more than twenty years. Electrospun nanofibers have fiber diameters that are 5-10 times smaller than the smallest meltblown fibers available. Recently, Ultra-Web® nanofiber filter media from Donaldson Company has become available to the non-wovens and filtration industries for a broad range of filtration applications. Nanofibers provide dramatic increases in filtration efficiency at relatively small (and in some cases immeasurable) decreases in permeability. In many laboratory tests and actual operating environments, nanofiber filter media also demonstrate improved filter life and more contaminant holding capacity. Nanofiber filter media have enabled new levels of filtration performance in several diverse applications with a broad range of environments and contaminants. The performance of nanofiber media in a mining vehicle cabin air filter will be discussed.
Figure 1. Ultra-Web® Nanofiber Filter Media
where λ is the gas mean free path (the dimension of the non-continuous nature of the molecules), and rf is the radius of the fiber. When Kn becomes nonneglible, the continuous flow theory, which does not take into account the molecular nature of air, starts to become less valid. While there is no exact Kn above which slip flow will prevail, it generally needs to be considered when Kn > 0.1, and definitely needs to be considered when Kn is around 0.25. For air at standard conditions, the mean free path is 0.066 microns; therefore, for fibers with diameters smaller than 0.5 microns, slip flow must be considered. In
2003 Donaldson Company Inc.
nanofiber webs have been applied onto various substrates. the air velocity at the fiber surface is assumed to be non-zero. page 2 . the benefit of achieving better filter efficiency at the same pressure drop actually accelerates when fiber sizes are less than 0. and durability in use. 8].) with ISO Fine test dust. 4] in their valid range. interception and inertial impaction efficiencies. The thin web has limited mechanical properties that preclude the use of conventional web handling and filter pleating equipment. Therefore. and due to the benefit of having slip flow at the fiber surface. As a result. slip flow. due to the dependence of efficiency and pressure drop on fiber sizes. Substrates are often chosen to resemble conventional filter materials. ISO Fine test dust is commonly used for testing engine air cleaners. As the fibers themselves have a small diameter. A voltage is applied to the polymer solution. resulting in higher diffusion. Figure 1 is a photomicrograph of commerciallyavailable nanofibers electrospun onto a cellulose substrate for air filtration applications. Nanofiber web density can be adapted and controlled.Presented at the Nonwovens in Filtration .Fifth International Conference. nanofibers with diameters in the range of 40-2000 nm can be made. The filtration properties of nanofibers can also be shown visually by reviewing SEM’s of nanofiber media that have been exposed to contamination. 2. which has been described in the literature  and in patents . which translates into lower pressure drop. Figure 2 shows a very light layer of nanofibers.3 micron diameter are highly desired for filtration applications. The effects of slip flow on pressure drop and efficiency can be further illustrated by applying mathematical equations such as those by Stechkina and Pich [3. drag force on a fiber is smaller than that in the case of non-slip flow. METHOD FOR MAKING NANOFIBERS Polymeric nanofibers can be made using the electrospinning process. diameters approaching only one micron. Substrates are selected to provide appropriate mechanical properties to allow pleating. The nanofiber diameter is approximately 250 nanometers. which allows the use of conventional filter media pleating and element handling equipment. which can be collected on a web.g. filter fabrication. with diameters exceeding 10 microns. Figure 2. By choosing a suitable polymer and solvent system. EXAMPLES OF ELECTROSPUN NANOFIBERS Scanning electron micrographs (SEMs) are generally used to characterize electrospun nanofibers. Figure 3 shows a cellulose media and a cellulose/nanofiber composite media (with nanofibers on the upstream side). March 2003. This is a low density web.5” w. the thickness of the nanofiber web can likewise be quite small. The filtration properties of nanofibers have been discussed theoretically. Stuttgart. both of which have been loaded to the same pressure drop (0. Thus. although such results are not presented here as they are beyond the scope of this paper. the slip flow makes the portion of the air flowing near the fiber surface larger than that in the case of non-slip flow. Germany. Additionally. The fine jets dry to form polymeric fibers.2 to 0.5 microns. and 3. Electrospinning uses an electric field to draw a polymer solution from the tip of a capillary to a collector. and a process for making them has been described. which causes a jet of the solution to be drawn toward a grounded collector. Due to the slip at the fiber surface. small fiber sizes such as those of 0. as compared to the cellulosic fiber structure. On the other hand. with a thickness of four 250 nm nanofiber 2003 Donaldson Company Inc. The electrospinning process has been documented using a variety of fiber forming polymers [7. Controlling parameters of electrospinning allows the generation of webs with different filtration characteristics. which translates into more particles traveling near the fiber.
01 to 0. March 2003. Two gravimetric particle sampling devices were used on a Caterpillar 992G wheel loader. mining companies and government agencies such as the Mine Safety and Health Association (MSHA). one placed just inside the cab and the other just outside the cab.Fifth International Conference.5 times more mass of dust than the cellulose sample . with the salt particles. The nanofibers are covered 2003 Donaldson Company Inc. while the composite sample shows loading at the nanofiber surface and a significant quantity of submicron particles captured. This section will discuss some of the unique attributes of nanofibers through an examination of their performance. page 3 . Germany. with particles in the size range of 0. Increased filtration efficiency for submicron contaminants can be achieved with nanofibers.7 – 70 microns. ISO Fine loading on conventional cellulose media (top) and nanofiber media (bottom). Figure 4 shows a nanofiber composite media sample that has been exposed to a submicron sodium chloride contaminant. Recent work with mining equipment manufacturers and the MSHA has shown that nanofiber filter media can further reduce cabin dust concentration compared to standard (wet-laid cellulose) filter media [11.5 microns. The composite sample is holding 2. while the larger substrate fiber has collected relatively few of the submicron particles . The performance of standard cellulose intake and recirculation filters Figure 3. Stuttgart. Figure 4 Sun-micron salt crystals preferentially collect on nanofibers (compared to large spunbond fiber in upper left) due to smaller fiber diameter. Nanofiber Filter Media in Cabin Air Filtration of Mining Vehicles Airborne contamination in the personnel cabins of mining equipment is of concern to mining workers. contains particles in the size range of 0. both very near the cab fresh air filter. FILTRATION APPLICATIONS USING NANOFIBERS Nanofiber webs have been used in a variety of air filtration applications.Presented at the Nonwovens in Filtration . 12]. 4. The cellulose sample shows depth loading and relatively few submicron particles.
It can be seen that the increase in particle removal efficiency detailed in Figure 7 was achieved without a corresponding decrease in filter life or significant increase in initial pressure drop. thus providing an improvement in worker protection (Figure 5). panel filters were constructed to the same dimensions as those used in the field test: 26. Pennsylvania. The electrospinning process itself has many important technical parameters that must be understood and controlled.361 0.003 0.12” x 5.06 68% 86% Outside Dust mg/m3 Inside Dust mg/m3 Dust Reduction. were compared with composite cellulose/nanofiber intake and recirculation filters on subsequent days in August. and nanofiber web formation and characterization Quality control of the nanofiber web is also important.025 92% 93% Figure 5. 2003 Donaldson Company Inc. % Ultra-Web(R) sub-micron respirable (>1 micron) 0. containing 186 two-inch deep pleats.Presented at the Nonwovens in Filtration . and is presented in Figure 6. electrical field control. two containing the standard media and two with the high efficiency nanofiber media. These include polymer and solvent selection.037 0. (38 mm Aq). A significant increase in filter efficiency was observed with the installation of the nanofiber composite filters. Figure 6 Similar life with nanofiber filter and “standard” filter. A patented method has been successfully implemented to provide real-time information about web consistency in the both the machine and crossmachine direction .g. Anecdotal evidence from field trials supports the data presented here. Testing was terminated when the pressure drop of the filter element exceeded 1.01 0.37” x 2.Fifth International Conference. Pressure drop data as a function of the amount of dust fed was recorded. while nanofiber filter achieves substantial efficiency increase shown in Figure 5 5. traditional on-line QC methodologies used for conventional non-wovens may not be appropriate and novel methods have been developed . Germany. SAE Fine dust was fed at a rate of 2. 1998 at Kaufman North Pit in Clearfield County.5” w. Filter Cellulose sub-micron respirable (>1 micron) 0. Because of the small fibers and low basis weights. For life testing. PRODUCTION AND QUALITY CONTROL OF NANOFIBER WEBS The production process and quality control of electrospinning nanofiber webs present some special challenges. March 2003. page 4 .1 g/min to each filter element.031 0. Stuttgart. solvent evaporation and management.19”. Use of nanofiber filter resulted 4 times less penetration of sub-micron dust.441 0. Four filters were tested. which is the pressure drop at which mining cab filters are typically changed or cleaned.
Volume 31.P...  Chun. E. and Olson.. 1-8. Gibson. 2000 in Dallas. Chapter 1.  Formhals. K. 16].201 “On-line Web Filtration Efficiency Test Method” assigned to Donaldson Company Inc. June 1999.. R.H. Barris. B.. “Different electrostatic methods for making electret filters”. Air Filtration. Aerosol Technology.” Ann.  Schaefer. H. “Process and Apparatus for Preparing Artificial Threads”.  Schaefer. J.  Garcia. R. Nanotechnology for the Soldier System Conference. A. pages 216-233. Reneker. M. “Carbon Nanofibers from Polyacrylonitrile and Mesophase Pitch”. H. R. McDonald. Knauf..  Stechkina.B. Volume 54.Presented at the Nonwovens in Filtration . “Polymeric Nanofibers in Air Filtration Applications” Fifteenth Annual Technical Conference & Expo of the American Filtration & Separations Society. Journal of Advanced Materials.. Fuchs. A.. J. J. and Haney. 1996.  Presented by the Mine Safety and Health Administration (MSHA) at a training seminar “OneDay Metal/Nonmetal Seminar” held March 21.. 1-132... Vol. April 2002 REFERENCES  Hinds.A.  Luzhansky. J. Germany. M. M. edited by M.504. July 1998.. Schreuder-Gibson. Grafe.  Grafe. pages 36 – 41.M. J. Journal of Electrostatics.S. John Wiley & Sons.. H. I.. Hug. Army Research 2003 Donaldson Company Inc.  Reneker. Number 1.A. “Quality Control in Manufacturing of Electrospun Nanofiber Composites” presented at The Fiber Society Fall Technical Meeting. N. Oxford..C. Filtration & Separation. Produced by Electrospinning”....W.J. ACKNOWLEDGEMENTS Portions of this work were previously published [15. Nanotechnology. Laboratory (ARL). Cambridge. 1987.. R. D. A. X.A. 2002  Gogins. 1934.. Fang. Schaefer. K. P.  Tsai. P... H. Beck Tan.. 2001. Volume 7. M. 12. B. M... MA. March 1998. “Nanofibers in Aerosol Filtration”. Stuttgart. Gareis. Kearns.  Pich. “Gas filtration theory. 1982. “Nanofibers in Filtration Applications in Transportation”. Army Research Office (ARO). T. Filtration 2001 Conference Proceedings.. sponsored by the U.975. Pergamon Press. Kirsch and N. A. Texas. 2002.. “Nanometre Diameter Fibres of Polymer. Orr. 1969. and Gogins. I. “Air Filtration Media for Transportation Applications”. I. D.. and the National Science Foundation (NSF). New York.” Filtration -Principles and Practices.. Fong.C. Army Soldier Systems Command (SSCOM).. US Patent 5. McDonald. Proceedings of the 8th US Mine Ventilation Symposium..L. Occup.IV calculation of aerosol deposition in model filters in the range of maximum penetration. US Patent 1. T. J. University of Missouri at Rolla. January 1999.  Brown. Gogins. P. Deitzel. Matteson and C. “Studies on fibrous aerosol filter -. and Chun. October 2. Canepa. L.B. T. D. March 2003. M. page 5 .. J.W. W.. 1993. Ouyang.  Graham.Fifth International Conference. “Effectiveness of Cabs for Dust and Silica Control on Mobile Mining Equipment”. Raether. Gresh.203.
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